Harold j



to coal solutions. Coalplastios prepared in Patented Sept. 6, 1932 Q err-rice HAROLD J'. ROSE, 0F PENN TOWNSHIP, ALLEGHEN-Y COUNTY, PENNSYLVANIA; ,AND

WILLIAM H. HILL, OF ARLINGTON, JERSEY, ASSIGNORS' TO THE K OP PE BS COMPANY OEDEILAWARE A CORPORATION OF DELAWARE i p comrosrrrorr'or MATTER AND raocnssns or PREPARING THE snln no Drawing.

This invention relates to compositions 1 of are produced by the addition. of low boiling organic liquids; or,- so-called volatile solvents this'way are; adaptedto .dry- .out by evaporation: of the volatile solvent, leaving [the original coalsolutiom i In accordance with the present invention, a coal product of a coagulated nature and withcertain very desirable properties may be preparedby; theaddition of certain organic materials, other than volatile solvents, which. materials may be termed coagulating agents, since it has been-observed thatthe addition' of proper proportions ofthese materials to coal solutionstends-to convert dissolved coal into a suspensoid. I

A product" may be prepared which may be of a gelnature and whichmay assume agelatinous or 1' elly state; A- gel is a product of acoagulated j or plastic nature. and may be heredefinedasa colloidally: dispersed structure oonsisting of a; solid andia liquid phase or alsoof two viscousliquid phases, and having shape and cohesion, and, elastic properties, although 'it maybe veryrrich in liquid, There iresults a formation offiminute particles of undissolv'edcoal inthe coalsolvent'. A given mass of; treated coalj solution may contain somedissolved coal and particles of undissolved #coal 'or it may contain little or no. dissolved coal, in which vcase -substantiallyall of the previously. dissolved coal is changedtoa suspensoid. I

I When coagulat'ngagentsareajdded to coal solutions in the proper. proportions, it has been found that a product of a coagulated nature maybe formed havinga higher softening; point than-that of th'e'original coal solution, but retaining; a remarkable degree of softness. In other words, while the softening point of the product is higher thanthat of the original coal-solutiom the product retains-the low degree oi hardnesso-fthe Applicationflled' September-16; 1929; Serial No. 393,124;

original coal solution at low temperatures.

Thus the temperature susceptibility factor is greatly decreased by the addition of a co agulatingsubstance. p

The degree. of the effects produced, and described. above, "can be. controlled, and itdepends on the particular coagulating, agent added, on the amount of such agent, onthe temperature of the coal solution or of the coagulating. agent when about to be miXed,.onthe temperature to which the resulting mix ture' is is heated and: on the speed with which the coagulating agentris' added 7 The con? sistency of the final. product depends largely upon the above, factors.

The present 'nvention makes it possible to produce coagulated coal-solutions of: higher softening points-without increasing the coal content.- For instance', a given coal solution maybe found to possess exactly thedesired properties with respect to hardness at low temperatures but too low a softening; point. Formerly there was onlyone'method oi overcoming; this, that is, by-fincreasin'g the coal content of thesolutiorn This-generally results in the loss ofcertain properties inherent in solutions containing lesser amounts ofdissolved coal. The present invention makesfit possible to increase the softening' point to the desired higher temperatures without decreasinggthe percentage of} solvent and" still retain the desirable propertiesiof the un: treated c'oallsolution;

As set forth in the co ending application Serial No. 97,467 filed. ar, 25, 1926' by Bose andiHill, coal may beidissolved in oils such as coal tar or water-gas ta-rand certain,di stillates therefrom. .The coal and oil are brought, together and heated at normal or only moderately elevated pressures and mod erately elevated 'butnOn-decomposing ternperatures of fromabOutQOU C. toabout 400 Ci Substantially all of the coal dis: solves, forming. homogeneousv solutions which remain stable attemperatures'below the point of rapid volatilization or even below the dissolving temperatures.- The coals mosteasily dissolved ,insuch solvents are of Y such coals are soluble, the. insoluble portions consisting of the mineral matter or ash and the mineral charcoal or fusain which may be present in limited amounts.

Preferably a high boiling coke-oven-tar oil is used as a solvent for coal. Other oils such as cracked petroleum oils, and especially the higher boiling distillates thereof may also be used. 7 v p r A coal solution may be prepared by heat ng one part of coal, such as Pittsburgh seam coal, and about three parts of crude coke-oven tar, for instance, in a closed vessel heated directly to a temperature of about 300 (1, or below the temperature at which substantial decomposition of the coal takes place. WVater and undesirable light oils are allowed to escape before the vessel is closed. The resulting product containing coal which is chemically unchanged, is allowed to cool and is discharged into containers at a temperature lower than the lowest boiling temperature (about 200 C'.) of compounds contained therein. i

i In addition to the solventsfor coal mentioned above, sulphur treated oils and tars described in the copending application of Rose and Hill, Serial No. 354,694, filed April 12, 1929, may also be used.

In accordance with the present process, a coal solution is prepared by dissolving coal in any of the solvents mentioned above, and anydesired proportions of coagulating materials or reagents may be added to the resulting coal solution with stirring or kneading.

The exact percentage of coagulating materials to be added depends upon the nature of the coal solution and the coagulating material and also upon the properties desired in the final product. Preferably. and in most cases. from about 1% to about 5% ofcoagulating materials may be added to a coal solution.

The coagulating materials, used are pre ferablv compounds of, or substances containing compounds of. the aliphatic series. such as paraffin oil. paraffin wax, lubricating oil, petroleum still residue, natural or blown asphalts. linseed oils. etc. It is desirable to employ coagulating materials of such high boilim points that they-do not evaporate materiallvafter the coagulated product has been ap lied.

In the use of drying oils such as linseed oil, une oil or so-called Chinese wood oil. and so forth, as coagulating materials,it is noted that aproduct prepared with such oils becomes covered by a dense tough impermeable film of oxidized drying oil which is very achantageous in that it effectively reduces evaporation of the oils used as solvents for coal or other alterations in the coagulated coal solutions and thus reduces ageing to a minimum. As an alternative, a product of thisinvention may be prepared by mixing a coagulating material with a solvent for coal, adding coal thereto and heating the resulting mixture.

Some examples of the manner in which the products of this invention may be prepared are as follows:

Example 1.95 parts by weight of coal solution containing 15% by weight of coal are melted and into it are slowly introduced with vigorous stirring 5 parts by weight of linseed oil. I

Example 2-80 parts by weight of cokeoven tar, topped to 400 F., and ,5 parts by weight of paraffin oil are mixed and heated for two hours with 15. parts by weight of bituminous coal in a rotating autoclave at 610 F. The product is ready for use after it has cooled down to less than about 400 F. Various inorganic and organic materials may be added to such coal solution products. The added materialsmay be of a purely inert type, as for instance pigments and fibres, such as clay, sand, mineral wool, asbestos, cellulose fibre, etc.;- or they may exert some chemical or physical action, as for instance sulphur or its compounds.

Coagulated masses produced in accordance with the present invention may be called nonevaporative coagulated coal solutions. They are usually thickened coal solutions of a solid,

semisolid, plastic or-semi-plastic nature and may be applied asa cold plaster or paste in thick layers without danger of drying out while preparing and applying them, or they may be applied as hot liquids. -However, they may vary inconsistency from a liquid toa solid and may be readily applied with a trowel, a putty knife or similar'instrument without the use of heat.

A composition having'remarkable elastic qualities may be produced which is particularly useful in the preparation of expansion joints. Non-evaporative coal gels or-coagulated coal solutions may also be used as patching compounds for roofs, etc., or they may be used for renewingbrake surfaces or in building up wearing surfaces.-' These products have excellent protective qualities and may be used as a Water-proofing agent, as for instance, on ships decks and so forth.

WVe claim as our invention: 0

1. A process of preparing bituminous proclucts, which process comprises heating coal and oil solvent for coal together to non-decomposing temperatures of the coal, namely about 200 C. to 400 C., to form a homogeneous fluid mass, maintaining the said mass in a fluid state, and mixing with the said mass a composition of aliphatic nature selected from a group consisting of vegetable oil, paraffin oil, parafiin wax, lubricating oil, petroleumstill residue, and asphalt in sufficient amount to form a thickened mass upon addition thereof.

2. A process of preparing bituminous products, which process comprises heating coal and oil solvent for coal together in the form of a homogeneous fluid mass at a temperature below the temperature at which chemical decomposition of the coal takes place and mixing with the said fluid mass acomposition of aliphatic nature selected from a group consisting of vegetable oil, paraflin oil, parafiin wax, lubricating oil, petroleumstill residue, and asphalt in sufficient amount to form a thickened mass upon addition thereof.

3. A bituminous productcomprising coal and solvent for coal which have been heated together to non-decomposing temperatures of about 200 O.'to 400 (1., and a composition of aliphatic nature selected from a group consisting of vegetable oil Jaraflinoil, parafiin wax, lubricating oil, petroleum still resi due, and asphalt in sufficient amount to form a thickened mass upon addition thereof.

4. A bituminous product comprising previously dissolved coal uniformly distributed in a solvent for the coal, and linseed oil dis tributed in the solvent in sufficient amount to cause separating out of coal from solution and to form a thickened mass upon addition of the said linseed oil.

5. A process of preparing bituminous products, which process comprises heating coal and oil solvent for coal together to non-decomposing temperatures of the coal, namely about 200 C. to 400 (1, to form a homogeneous fluid mass, and thickening the said fluid mass by adding a relatively high-boiling liquid aliphatic composition'which when added will" increase the consistency of the said fluid mass while distributing the said composition in the said fluid mass.

In testimony whereof,- I have hereunto sub scribed my name this 5th day of September,

V HAROLD J ROSE. In testimony whereof, I have hereunto subscribed my name this 9th day of. September,

WILLIAM H. HILL. 

